苯硼酸双柱固相微萃取-超高效液相色谱-串联质谱分析单胺类神经递质

本文构建了苯硼酸双柱固相微萃取-超高效液相色谱-串联质谱分析3种单胺类神经递质的方法。苯硼酸固相微萃取柱以4-乙烯基苯硼酸和甲叉双丙烯酰胺原位聚合法制备,该介质对含有顺式二羟基分子的化合物能够进行特异性捕获,并采取扫描电镜,红外光谱对其进行表征,研究了影响富集的各种条件。在优化条件下,线性度好,相关系数大于0.9971,检出限为23.6~152 pmol·L^-1,相对标准偏差(RSD)不大于5.9%。采用该方法对人体尿液和大鼠血清样品中3种单胺类神经递质进行分析,加标回收率为82.9%~113%,RSD为2.6%~7.7%。本文方法分析效率高,灵敏度高,准确度好,适用于尿液和大鼠血清样品中痕量单胺类神经递质的测定。

Determination of monoamine neurotransmitters by dual monolithic column solid-phase microextraction based on boronate affinity coupled with UHPLC-MS/MS

A novel method based on boronate affinity tandem dual monolithic column solid-phase microextraction coupled with UHPLC-MS/MS was developed for the analysis of three Monoamine neurotransmitters(MNTs).The boronate affinity monolithic column was prepared by in situ polymerization of 4-vinylphenylboronic acid and N,N-methylenebisacrylamide,it is a powerful sorbent for specific extraction of cis-diol-containing compounds.The monolithic column was investigated by scanning electron microscopy and infrared spectroscopy analysis.Under the optimized conditions,the developed method exhibited low limit of detection(23.6~152 pmol),good linearity(with R² greater than 0.9971)and relative standard deviations(RSD)no more than 5.9%.The proposed method was successfully applied in the determination of MNTs in human urine and rat serum samples,with recoveries of 82.9%~113%and RSDs of 2.6%~7.7%.The analytical method was rapid,sensitive,and accurate for analyzing trace MNTs in human urine and rat serum.